Method for nitrogen-assisted segmented directional extraction of aromatic plant hydrolat

Abstract

The invention relates to the technical field of aromatic plant hydrolat production processes, and discloses a method for nitrogen-assisted segmented directional extraction of aromatic plant hydrolat in order to solve the problem of low content of aromatic components and functional components in an aromatic plant hydrolat product in an existing process for extracting aromatic plant hydrolat by a steam distillation method. Comprising the following steps: mixing fresh aromatic plant petals with pure water, and adding adsorption particles to obtain a distilled mixture; placing the distilled mixture in a nitrogen environment, heating and pressurizing, distilling, and condensing to recover a distillate; and continuously introducing hot air at 80-120 DEG C, and collecting distillate to obtain the aromatic plant hydrolat. Nitrogen is introduced to prevent the raw materials from being in contact with oxygen in the air in the distillation process and being subjected to oxidation reaction in a heating environment, so that the aromatic plant hydrolat product has peculiar smell after being cooked; meanwhile, through precise pressure control, the volatilization loss of water vapor in the distillation process can be reduced, so that the purpose of retaining and concentrating effective components is achieved.

Description

Technical Field

[0001] The present invention relates to the technical field of the production process of aromatic plant hydrosols, and more specifically, to a method for nitrogen-assisted segmented directional extraction of aromatic plant hydrosols. Background Art

[0002] Aromatic plant hydrosol refers to the saturated distillation stock solution separated during the extraction of essential oils from aromatic plants. It is a by-product of essential oil preparation, with natural ingredients, a light fragrance, and functions such as moisturizing. In current industrial production, steam distillation is mainly used to extract and prepare aromatic plant hydrosols. By heating and pressurizing, the active ingredients in the petals of aromatic plants are extracted, and the large amount of volatile substances contained therein can endow the aromatic plant hydrosols with special fragrances and effects.

[0003] For example, the patent with the publication number CN115161114A proposes a method for extracting hydrosol from spliced roses of different varieties. The roses of different varieties are mixed and crushed in proportion, then mixed with distilled water, and after two distillation treatments, products of rose hydrosol and rose essential oil are obtained. The sensory evaluation such as the fragrance of the rose hydrosol product is enriched and improved by mixing raw materials of multiple varieties of roses.

[0004] However, during the preparation process, the aromatic substances in the aromatic plant raw materials volatilize with the water during distillation, resulting in a low content of these volatile components, making the aroma of the product not strong enough, the efficacy weak, and restricting the application and promotion of the product. In addition, some harmful volatile components in aromatic plants will also be distilled out and mixed in the hydrosol. For example, components such as methyl eugenol contained in many aromatic plants have a certain carcinogenic effect. Summary of the Invention

[0005] The purpose of the present invention is to solve the problem of low content of aromatic components and efficacy components in the aromatic plant hydrosol products existing in the existing process of extracting aromatic plant hydrosols by steam distillation, and can purify the aromatic plant hydrosol, playing a role in directionally removing harmful components.

[0006] The present invention is achieved through the following technical solutions:

[0007] The present invention provides a method for nitrogen-assisted segmented directional extraction of aromatic plant hydrosols, including the following steps:

[0008] S1 Take fresh aromatic plant petals and mix them with pure water, add adsorption particles to obtain a distillation mixture;

[0009] S2 Place the distillation mixture in a nitrogen environment, heat and pressurize, carry out distillation, and condense and recover the distillate;

[0010] S3 Continuously introduce hot air at 100 - 120 °C, collect the distillate to obtain the aromatic plant hydrosol.

[0011] Preferably, in step S1, the material ratio of fresh aromatic plant petals to pure water is 1 g: 3-10 mL, and the adsorption particles account for 5-18 wt% of the total mass of fresh aromatic plant petals and pure water.

[0012] Preferably, in step S2, first pressurize to above 0.02 MPa; then heat and distill, and continuously introduce nitrogen. During the heating and distillation, control the pressure to be 0.02-0.12 MPa.

[0013] Preferably, the heating and distillation include primary distillation, secondary distillation and tertiary distillation; the pressure of primary distillation is 0.02-0.06 MPa, the distillation temperature is 80-90 °C, and the time is 20-30 min; the pressure of secondary distillation is

[0014] 0.06-0.10 MPa, the distillation temperature is 90-110 °C, and the time is 30-45 min; the pressure of tertiary distillation is 0.10-0.12 MPa, the distillation temperature is 110-120 °C, and the time is 20-40 min. By controlling the extraction temperature and pressure, the volatile components in the aromatic plants can be distilled out in segments, achieving the purpose of purification and directional extraction.

[0015] Preferably, in step S3, the treatment time of continuously introducing hot air is 40-120 min.

[0016] Preferably, in step S1, the adsorption particles include activated carbon particles, zeolite and silica gel microparticles.

[0017] Preferably, by mass fraction, the sum of the masses of activated carbon particles and zeolite accounts for 60-78% of the total mass of the adsorption particles, and the mass ratio of activated carbon particles to zeolite is 1.5-2.5: 1-1.5.

[0018] Preferably, the preparation method of the adsorption particles includes the following steps:

[0019] Take activated carbon particles and zeolite, mix them evenly, then add silica gel microparticles, disperse them by ultrasonic wave, evacuate to 0.02-0.05 MPa, and let it stand to obtain the adsorption particles.

[0020] The technical solution of the present invention has the following beneficial effects:

[0021] The method for nitrogen-assisted segmented and directional extraction of aromatic plant hydrosol in the present invention avoids the contact between the raw materials and oxygen in the air during the distillation process by filling nitrogen, and prevents oxidation reactions from occurring in a heating environment, which would cause the aromatic plant hydrosol product to have an unpleasant smell after cooking. At the same time, through precise pressure control, not only can the volatilization and loss of water vapor during the distillation process be reduced, the extraction rate of the active ingredients being carried out be accelerated, and the purpose of retaining and concentrating the active ingredients be achieved, but also the volatile components in the aromatic plants can be controlled to be distilled out in segments by controlling the extraction temperature and pressure, achieving the purpose of purification and directional extraction. In addition, the present invention also adsorbs the active ingredients during the distillation process to prevent them from being lost with the water vapor. After the distillation is completed, the active ingredients are separated by thermal desorption and then condensed and collected into the distillation extract, so as to extract and collect the active ingredients in the aromatic plants to a greater extent. Detailed implementation manners

[0022] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Among them, for those conditions not specified in the embodiments, they are carried out according to conventional conditions or the conditions recommended by the manufacturer; for those instrument devices, reagent raw materials, etc. whose manufacturers are not specified, they are all conventional products that can be obtained through commercial purchase.

[0023] The present invention provides a method for nitrogen-assisted segmented and directional extraction of aromatic plant hydrosol. Taking rose petals as an example, the method includes the following steps:

[0024] (1) Mix fresh rose flowers and pure water at a material-liquid ratio of 1 g: 3 - 10 mL, add them to a high-pressure distillation kettle, add adsorption particles, and the adsorption particles account for 5 - 18 wt% of the total mass of the above-mentioned materials, and control the materials in the kettle not to exceed 70% of the volume of the high-pressure distillation kettle;

[0025] Among them, the adsorption particles include activated carbon particles, zeolites, and silica gel microparticles. By adsorbing the active ingredients during the distillation process, it is possible to prevent them from being lost with the water vapor. After the distillation is completed, the active ingredients are separated by thermal desorption and then condensed and collected into the distillation extract, so as to extract and collect the active ingredients in the rose flowers to a greater extent.

[0026] (2) Introduce nitrogen into the high-pressure distillation kettle until all the air is exhausted; then close the high-pressure distillation kettle to form a sealed environment, and introduce nitrogen to raise the pressure in the kettle to 0.02 MPa or above.

[0027] (3) Heat and distill the content in the high-pressure distillation kettle, continuously introduce nitrogen during this period, control the pressure in the kettle to be maintained at 0.02 - 0.6 MPa, the distillation temperature to be controlled at 80 - 90 °C, and the distillation time to be 20 - 30 min, and collect the first distillate.

[0028] (4) Continue heating and introduce nitrogen gas. Control the pressure in the autoclave to be 0.06 - 0.10 MPa, and control the distillation temperature at 90 - 110 °C for secondary distillation. The distillation time is 30 - 45 min, and the secondary distillate is recovered by condensation through the distillation tube.

[0029] (5) Continue heating and introduce nitrogen gas. Control the pressure in the autoclave to be 0.10 - 0.12 MPa, and control the distillation temperature at 110 - 120 °C for tertiary distillation. The distillation time is 20 - 40 min, and the tertiary distillate is recovered by condensation through the distillation tube.

[0030] (6) Extract the remaining pure water in the high-pressure distillation autoclave, introduce hot air at 100 - 120 °C, and ventilate continuously for 40 - 120 min. During this period, keep the distillation tube connected to the high-pressure distillation autoclave and the distillate container respectively, and place the distillate container in a cold water bath.

[0031] In the present invention, the condensed nitrogen gas can be dried and then reused in the nitrogen generator to reduce resource consumption and production costs. After the above treatment, the rose hydrosol obtained in the distillate container has the characteristics of rich aroma and no cooking odor. The contents of aromatic components and functional components are high, and no other elemental substances are introduced during the extraction process, which can maintain the purity and safety of the product and has low production costs.

[0032] In the present invention, the preparation method of the adsorption particles includes the following steps:

[0033] Take activated carbon particles and zeolite, mix them evenly, then add silica gel microparticles, ultrasonically disperse for 25 - 40 min, evacuate to 0.02 - 0.05 MPa, and let stand for 10 - 25 min to obtain the above-mentioned adsorption particles.

[0034] Among them, by mass fraction, the sum of the masses of the activated carbon particles and zeolite accounts for 60 - 78% of the total mass of the adsorption particles, and the mass ratio of the activated carbon particles to zeolite is preferably 1.5 - 2.5:1 - 1.5.

[0035] Example 1

[0036] Step 1: Take 62.4 g of activated carbon and 40.3 g of zeolite respectively, and control their particle sizes within 2.5 - 5 mm, stir and mix evenly; then add 45.8 g of silica gel microparticles mainly composed of SiO2, with a particle size of about 0.6 ± 3 mm, ultrasonically disperse for 35 min, then place it in a sealed vacuum chamber, evacuate to about 0.03 MPa, let stand for 20 min, take out, which is the adsorption particles for standby.

[0037] Step 2: Separately take about 200 g of fresh roses and 1200 mL of pure water, add them together into a 2.5 L high-pressure distillation kettle, then add the above-mentioned adsorption particles, and then close the high-pressure distillation kettle. Introduce nitrogen into the kettle until the air is exhausted and the pressure in the kettle exceeds 0.02 MPa.

[0038] Step 3: While continuously introducing nitrogen, heat until the materials in the kettle are in a slightly boiling state for distillation. During this period, control the pressure in the kettle to be about 0.04 ± 0.02 MPa and the temperature to be 80 - 90 °C for 25 minutes of primary distillation; then continue to control the pressure in the kettle to be 0.08 ± 0.02 MPa and the temperature to be 90 - 110 °C for 30 minutes of secondary distillation, and then control the pressure in the kettle to be 0.11 ± 0.01 and the temperature to be 110 - 120 °C for 30 minutes of tertiary distillation, and condense and recover the distillate.

[0039] Step 4: Keep the condenser and the distillate in communication with the high-pressure distillation kettle, draw out the remaining distillation liquid in the kettle, and then continuously introduce hot air at 120 °C from the bottom of the kettle for 75 minutes of continuous ventilation. The hot air flows through the condenser to the distillate, and the finally collected secondary and tertiary distillates are the rose hydrosol.

[0040] Example 2

[0041] Step 1: Separately take 65.3 g of activated carbon and 40.5 g of zeolite, and control their particle sizes to be within 2.5 - 5 mm, stir and mix evenly; then add 48.2 g of silica gel particles mainly made of SiO2 with a particle size of about 0.6 ± 3 mm, ultrasonically disperse for 35 minutes, and then place them in a sealed vacuum chamber, evacuate to about 0.03 MPa, stand for 20 minutes, take out, and it is the adsorption particles for standby.

[0042] Step 2: Separately take about 150 g of fresh roses and 1150 mL of pure water, add them together into a 2.5 L high-pressure distillation kettle, then add the above-mentioned adsorption particles, and then close the high-pressure distillation kettle. Introduce nitrogen into the kettle until the air is exhausted and the pressure in the kettle exceeds 0.02 MPa.

[0043] Step 3: While continuously introducing nitrogen, heat until the materials in the kettle are in a slightly boiling state for distillation. During this period, control the pressure in the kettle to be about 0.04 ± 0.02 MPa and the temperature to be 80 - 90 °C for 25 minutes of primary distillation; then continue to control the pressure in the kettle to be 0.08 ± 0.02 MPa and the temperature to be 90 - 110 °C for 30 minutes of secondary distillation, and then control the pressure in the kettle to be 0.11 ± 0.01 and the temperature to be 110 - 120 °C for 30 minutes of tertiary distillation, and condense and recover the distillate.

[0044] Step 4: Keep the condenser and the distillate both connected to the high-pressure distillation kettle, draw out the remaining post-distillation liquid in the kettle, then continuously introduce hot air at 120°C from the bottom of the kettle, ventilate continuously for 75 minutes, the hot air flows through the condenser to the distillate, and finally collect the distillate of the second and third times, which is the rose hydrosol.

[0045] Example 3

[0046] Step 1: Take 58.0 g of activated carbon and 45.6 g of zeolite respectively, and control their particle sizes to be within 2.5 - 5 mm, stir and mix evenly; then add 50.2 g of silica gel particles with SiO2 as the main raw material, with a particle size of about 0.6 ± 3 mm, disperse ultrasonically for 35 minutes, then place them in a sealed vacuum chamber, evacuate to about 0.03 MPa, let stand for 20 minutes, take out, and they are the adsorption particles for standby.

[0047] Step 2: Take about 120 g of fresh roses and 1050 mL of pure water respectively, add them together to a 2.5 L high-pressure distillation kettle, then add the above adsorption particles, then close the high-pressure distillation kettle, introduce nitrogen into the kettle until the air is exhausted and the pressure in the kettle exceeds 0.02 MPa.

[0048] Step 3: While continuously introducing nitrogen, heat until the materials in the kettle are in a slightly boiling state and carry out distillation. During this period, control the pressure in the kettle to be about 0.06 ± 0.02 MPa and the temperature to be 70 - 80°C for the first distillation for 25 minutes; then continue to control the pressure in the kettle to be 0.09 ± 0.01 MPa and the temperature to be 80 - 100°C for the second distillation for 30 minutes, and then control the pressure in the kettle to be 0.1 ± 0.01 and the temperature to be 100 - 110°C for the third distillation for 30 minutes, and condense and recover the distillate.

[0049] Step 4: Keep the condenser and the distillate both connected to the high-pressure distillation kettle, draw out the remaining post-distillation liquid in the kettle, then continuously introduce hot air at 120°C from the bottom of the kettle, ventilate continuously for 75 minutes, the hot air flows through the condenser to the distillate, and finally collect the distillate of the second and third times, which is the rose hydrosol.

[0050] Comparative Example 1

[0051] Step 1: Take about 200 g of fresh roses and 1200 mL of pure water respectively, add them together to a 2.5 L high-pressure distillation kettle, then close the high-pressure distillation kettle and introduce air for circulation.

[0052] Step 2: While continuously introducing air circulation, heat until the materials in the kettle are in a slightly boiling state, and perform distillation for 25 minutes. Then, continue to control the pressure in the kettle at 0.04 ± 0.01 MPa for secondary distillation for 30 minutes. Then, control the pressure in the kettle at 0.8 ± 0.01 and the temperature at 110 - 120 °C for tertiary distillation for 30 minutes, and condense and recover the secondary and tertiary distillates.

[0053] Step 3: Keep the condenser and the distillate in communication with the high-pressure distillation kettle, draw out the remaining post-distillation liquid in the kettle, and then continuously introduce hot air at 120 °C from the bottom of the kettle for 75 minutes. The hot air flows through the condenser to the distillate, and the finally collected distillate is the rose hydrosol.

[0054] Test Example

[0055] Use the rose hydrosols prepared in Examples 1 to 3 and Comparative Example 1 as samples, and measure the content of active ingredients in the samples respectively. The results are summarized in Table 1 below:

[0056] Table 1 Test Results of Active Ingredient Contents in Different Samples

[0057]

[0058] As can be seen from the above table, for the rose hydrosols prepared in Examples 1 to 3, the total content of active ingredients in the products is significantly higher than that of the rose hydrosol prepared by the traditional production method in Comparative Example 1; and among the total active ingredients, the total content of beneficial ingredients such as aromatic substances in the rose hydrosols prepared in Examples 1 to 3 accounts for more than half, and is significantly higher than the total content of beneficial ingredients in the rose hydrosol of Comparative Example 1. Moreover, the content of beneficial ingredients in the secondary-distilled rose hydrosols prepared in Examples 1 to 3 is significantly higher than that in the tertiary-distilled rose hydrosols, and is significantly higher than the content of beneficial ingredients in the tertiary-distilled rose hydrosol of Comparative Example 1. Therefore, it shows that by using the aromatic plant hydrosol extraction method proposed in the present invention, the extraction degree of active ingredients in aromatic plant raw materials can be effectively improved, so that a large amount of beneficial substances such as aromatic components are more retained in the aromatic plant hydrosol products, and the active ingredients in the rose hydrosol can be enriched in a segmented and directional manner, thereby making it have a more prominent characteristic aroma and higher purity quality.

[0059] The above are only the preferred embodiments of the present invention and are not used to limit the present invention. For those skilled in the art, the present invention can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for nitrogen-assisted segmented directional extraction of hydrosol from aromatic plants, characterized in that, It includes the following steps: S1: Mix fresh aromatic plant petals with pure water, and add adsorption particles to obtain a distillation mixture; S2: Place the distillation mixture in a nitrogen environment, heat and pressurize it, conduct distillation, and condense and recover the distillate; S3: Continuously introduce hot air at 80 - 120 °C, collect the distillate, and obtain pure aromatic plant hydrosol.

2. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to claim 1, characterized in that, In step S1, the material ratio of fresh aromatic plant petals to pure water is 1 g: 3 - 10 mL, and the adsorption particles account for 5 - 18 wt% of the total mass of fresh aromatic plant petals and pure water.

3. The method for nitrogen-assisted segmented and directional extraction of pure aromatic plant hydrosol according to claim 1, characterized in that, In step S2, first pressurize to above 0.02 MPa; then heat and distill, and continuously introduce nitrogen. During the heating and distillation process, control the pressure at 0.02 - 0.12 MPa.

4. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to claim 3, characterized in that The heating and distillation include primary distillation, secondary distillation, and tertiary distillation; The primary distillation pressure is 0.02 - 0.06 MPa, the distillation temperature is 80 - 90 °C, and the time is 20 - 30 min; The secondary distillation pressure is 0.06 - 0.10 MPa, the distillation temperature is 90 - 110 °C, and the time is 30 - 45 min; The tertiary distillation pressure is 0.10 - 0.12 MPa, the distillation temperature is 110 - 120 °C, and the time is 20 - 40 min.

5. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to claim 1, characterized in that, In step S3, the treatment time of continuously introducing hot air is 40 - 120 min.

6. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to any one of claims 1 to 5, characterized in that, In step S1, the adsorption particles include activated carbon particles, zeolite, and silica gel microparticles.

7. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to claim 6, characterized in that, By mass fraction, the sum of the masses of activated carbon particles and zeolite accounts for 60 - 78% of the total mass of the adsorption particles, and the mass ratio of activated carbon particles to zeolite is 1.5 - 2.5: 1 - 1.

5.

8. The method for nitrogen-assisted segmented directional extraction of pure aromatic plant hydrosol according to claim 6, characterized in that, The preparation method of the adsorption particles includes the following steps: Take activated carbon particles and zeolite, mix them evenly, then add silica gel microparticles, disperse them by ultrasonic wave, evacuate to 0.02 - 0.05 MPa, and let it stand to obtain the adsorption particles.

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